# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Martyn Coles' 'Peter B. Hitchcock' 'Majid S. Khalaf' 'Sarah H. Oakley' _publ_contact_author_name 'Martyn Coles' _publ_contact_author_email M.P.COLES@SUSSEX.AC.UK _publ_section_title ; Methylene bridged bis-guanidyls: contrasting coordination behaviour at palladium ; _publ_requested_category FM # Attachment 'Combined.cif' data_(1)-nov604 _database_code_depnum_ccdc_archive 'CCDC 743945' _audit_creation_date 2004-11-10T15:25:02-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C16 H29 Cl N6 Pd' _chemical_formula_sum 'C16 H29 Cl N6 Pd' _chemical_formula_weight 447.3 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 10.9381(3) _cell_length_b 11.6842(4) _cell_length_c 14.1258(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1805.32(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 26957 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.646 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.187 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8939 _exptl_absorpt_correction_T_max 1.0304 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.775756E-1 _diffrn_orient_matrix_ub_12 0.12681E-2 _diffrn_orient_matrix_ub_13 0.37445E-1 _diffrn_orient_matrix_ub_21 -0.48359E-1 _diffrn_orient_matrix_ub_22 -0.2782E-3 _diffrn_orient_matrix_ub_23 0.600776E-1 _diffrn_orient_matrix_ub_31 0.13068E-2 _diffrn_orient_matrix_ub_32 -0.855758E-1 _diffrn_orient_matrix_ub_33 0.3595E-3 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0782 _diffrn_reflns_av_unetI/netI 0.0462 _diffrn_reflns_number 28540 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.43 _diffrn_reflns_theta_max 26.05 _diffrn_reflns_theta_full 26.05 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 3570 _reflns_number_gt 3221 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The H atoms on C8 were refined; other H atoms were in riding mode. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0231P)^2^+1.7753P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 3570 _refine_ls_number_parameters 224 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0434 _refine_ls_R_factor_gt 0.034 _refine_ls_wR_factor_ref 0.0657 _refine_ls_wR_factor_gt 0.0628 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(4) _refine_diff_density_max 0.399 _refine_diff_density_min -0.439 _refine_diff_density_rms 0.081 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.19281(3) 0.71577(2) 0.24045(2) 0.01952(9) Uani 1 1 d . . . Cl Cl 0.38050(9) 0.80698(9) 0.23709(9) 0.0364(3) Uani 1 1 d . . . N1 N 0.2422(3) 0.6054(3) 0.1239(2) 0.0212(8) Uani 1 1 d . . . N2 N 0.0576(3) 0.6072(3) 0.0391(2) 0.0205(8) Uani 1 1 d . . . N3 N 0.1908(4) 0.4513(3) 0.0257(2) 0.0249(8) Uani 1 1 d . . . N4 N -0.0820(3) 0.7149(3) 0.1407(2) 0.0207(7) Uani 1 1 d . . . N5 N 0.0327(2) 0.6245(2) 0.2569(3) 0.0185(7) Uani 1 1 d . . . N6 N -0.1811(3) 0.6155(2) 0.2616(2) 0.0216(7) Uani 1 1 d . . . C1 C 0.1655(4) 0.5548(4) 0.0657(3) 0.0212(10) Uani 1 1 d . . . C2 C -0.0307(4) 0.5481(4) -0.0215(3) 0.0270(10) Uani 1 1 d . . . H2A H -0.0868 0.6044 -0.0507 0.032 Uiso 1 1 calc R . . H2B H -0.08 0.4942 0.0169 0.032 Uiso 1 1 calc R . . C3 C 0.0371(4) 0.4836(4) -0.0975(3) 0.0312(12) Uani 1 1 d . . . H3A H -0.0215 0.444 -0.1397 0.037 Uiso 1 1 calc R . . H3B H 0.0865 0.5371 -0.1362 0.037 Uiso 1 1 calc R . . C4 C 0.1186(4) 0.3982(4) -0.0495(3) 0.0310(11) Uani 1 1 d . . . H4A H 0.068 0.3361 -0.0223 0.037 Uiso 1 1 calc R . . H4B H 0.1743 0.3637 -0.0968 0.037 Uiso 1 1 calc R . . C5 C 0.2720(4) 0.3703(4) 0.0735(4) 0.0368(12) Uani 1 1 d . . . H5A H 0.3329 0.3412 0.0276 0.044 Uiso 1 1 calc R . . H5B H 0.2234 0.3043 0.0962 0.044 Uiso 1 1 calc R . . C6 C 0.3375(4) 0.4226(4) 0.1555(3) 0.0360(12) Uani 1 1 d . . . H6A H 0.4163 0.383 0.1661 0.043 Uiso 1 1 calc R . . H6B H 0.2875 0.4154 0.2136 0.043 Uiso 1 1 calc R . . C7 C 0.3594(4) 0.5466(4) 0.1333(3) 0.0286(11) Uani 1 1 d . . . H7A H 0.4078 0.5822 0.1847 0.034 Uiso 1 1 calc R . . H7B H 0.4063 0.5534 0.0737 0.034 Uiso 1 1 calc R . . C8 C 0.0204(4) 0.7191(4) 0.0734(3) 0.0213(8) Uani 1 1 d . . . H8A H -0.003(4) 0.768(4) 0.021(3) 0.026 Uiso 1 1 d . . . H8B H 0.095(4) 0.758(3) 0.100(3) 0.026 Uiso 1 1 d . . . C9 C -0.0750(3) 0.6499(3) 0.2217(3) 0.0186(9) Uani 1 1 d . . . C10 C -0.2016(4) 0.7576(4) 0.1097(3) 0.0283(10) Uani 1 1 d . . . H10A H -0.1958 0.7858 0.0438 0.034 Uiso 1 1 calc R . . H10B H -0.2271 0.8222 0.1505 0.034 Uiso 1 1 calc R . . C11 C -0.2957(4) 0.6627(4) 0.1153(3) 0.0337(11) Uani 1 1 d . . . H11A H -0.3765 0.6915 0.0947 0.04 Uiso 1 1 calc R . . H11B H -0.2719 0.5987 0.0732 0.04 Uiso 1 1 calc R . . C12 C -0.3024(4) 0.6217(4) 0.2165(3) 0.0268(10) Uani 1 1 d . . . H12A H -0.3551 0.6744 0.2533 0.032 Uiso 1 1 calc R . . H12B H -0.3407 0.545 0.218 0.032 Uiso 1 1 calc R . . C13 C -0.1860(4) 0.5590(4) 0.3544(3) 0.0262(9) Uani 1 1 d . . . H13A H -0.2098 0.4779 0.3458 0.031 Uiso 1 1 calc R . . H13B H -0.249 0.5964 0.394 0.031 Uiso 1 1 calc R . . C14 C -0.0649(4) 0.5645(4) 0.4042(3) 0.0285(11) Uani 1 1 d . . . H14A H -0.0624 0.5075 0.4561 0.034 Uiso 1 1 calc R . . H14B H -0.0528 0.6415 0.432 0.034 Uiso 1 1 calc R . . C15 C 0.0351(4) 0.5394(4) 0.3328(3) 0.0235(10) Uani 1 1 d . . . H15A H 0.1157 0.5411 0.3646 0.028 Uiso 1 1 calc R . . H15B H 0.0231 0.462 0.3058 0.028 Uiso 1 1 calc R . . C16 C 0.1432(4) 0.8232(3) 0.3493(3) 0.0190(9) Uani 1 1 d . . . H16A H 0.1072 0.8932 0.3231 0.028 Uiso 1 1 calc R . . H16B H 0.2156 0.8428 0.3867 0.028 Uiso 1 1 calc R . . H16C H 0.0832 0.7847 0.3898 0.028 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.01791(14) 0.02101(14) 0.01964(14) 0.00127(14) -0.00188(14) -0.00281(13) Cl 0.0261(5) 0.0358(6) 0.0474(7) 0.0049(6) -0.0044(5) -0.0091(4) N1 0.0180(18) 0.027(2) 0.0189(19) -0.0025(16) -0.0011(15) 0.0023(16) N2 0.0196(18) 0.0233(19) 0.0186(18) 0.0012(15) -0.0035(14) 0.0014(15) N3 0.0295(19) 0.0243(18) 0.0210(17) -0.0042(14) -0.0026(18) 0.0048(18) N4 0.0162(16) 0.0261(18) 0.0199(17) 0.0062(18) 0.0018(13) 0.0036(18) N5 0.0153(15) 0.0213(15) 0.0188(17) 0.0050(17) -0.0015(16) -0.0002(12) N6 0.0148(15) 0.0282(16) 0.0219(16) 0.0066(15) -0.0013(18) -0.0024(13) C1 0.022(2) 0.024(2) 0.017(2) 0.0024(18) 0.0061(17) 0.0003(18) C2 0.017(2) 0.038(3) 0.026(2) -0.003(2) -0.0041(19) -0.002(2) C3 0.021(2) 0.053(3) 0.020(2) -0.011(2) -0.0004(19) -0.003(2) C4 0.026(2) 0.036(3) 0.030(3) -0.012(2) 0.002(2) -0.003(2) C5 0.037(3) 0.025(3) 0.048(3) 0.001(2) -0.006(2) 0.007(2) C6 0.027(3) 0.043(3) 0.038(3) 0.008(2) -0.009(2) 0.008(2) C7 0.020(2) 0.038(3) 0.028(3) -0.005(2) -0.0028(19) 0.004(2) C8 0.017(2) 0.028(2) 0.018(2) 0.002(2) 0.0020(16) 0.001(2) C9 0.017(2) 0.016(2) 0.023(2) 0.0022(17) 0.0016(17) -0.0002(17) C10 0.023(2) 0.037(3) 0.025(2) 0.0100(17) 0.0026(19) 0.012(2) C11 0.018(2) 0.052(3) 0.031(2) 0.006(2) -0.006(2) 0.002(2) C12 0.017(2) 0.031(2) 0.033(2) 0.0029(18) -0.001(2) -0.003(2) C13 0.026(2) 0.029(2) 0.023(2) 0.0052(18) 0.003(2) -0.006(2) C14 0.027(2) 0.035(3) 0.023(2) 0.008(2) 0.001(2) -0.003(2) C15 0.020(2) 0.026(2) 0.025(2) 0.0043(19) -0.0014(18) -0.0028(19) C16 0.021(2) 0.016(2) 0.020(2) -0.0021(16) 0.0062(17) 0.0025(17) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd C16 2.057(4) . ? Pd N5 2.064(3) . ? Pd N1 2.161(3) . ? Pd Cl 2.3137(10) . ? N1 C1 1.315(5) . ? N1 C7 1.460(5) . ? N2 C1 1.382(5) . ? N2 C8 1.452(5) . ? N2 C2 1.463(5) . ? N3 C1 1.364(5) . ? N3 C4 1.462(5) . ? N3 C5 1.463(5) . ? N4 C9 1.376(5) . ? N4 C10 1.467(5) . ? N4 C8 1.470(5) . ? N5 C9 1.312(5) . ? N5 C15 1.462(5) . ? N6 C9 1.351(5) . ? N6 C13 1.469(5) . ? N6 C12 1.473(5) . ? C2 C3 1.507(6) . ? C3 C4 1.501(6) . ? C5 C6 1.492(6) . ? C6 C7 1.501(6) . ? C10 C11 1.514(6) . ? C11 C12 1.509(6) . ? C13 C14 1.501(6) . ? C14 C15 1.517(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C16 Pd N5 90.44(14) . . ? C16 Pd N1 178.61(15) . . ? N5 Pd N1 89.39(13) . . ? C16 Pd Cl 88.19(12) . . ? N5 Pd Cl 173.45(9) . . ? N1 Pd Cl 92.14(9) . . ? C1 N1 C7 113.9(3) . . ? C1 N1 Pd 125.8(3) . . ? C7 N1 Pd 115.5(3) . . ? C1 N2 C8 123.2(3) . . ? C1 N2 C2 120.9(3) . . ? C8 N2 C2 115.8(3) . . ? C1 N3 C4 124.6(4) . . ? C1 N3 C5 120.4(3) . . ? C4 N3 C5 112.9(3) . . ? C9 N4 C10 119.0(3) . . ? C9 N4 C8 120.9(3) . . ? C10 N4 C8 118.4(3) . . ? C9 N5 C15 116.6(3) . . ? C9 N5 Pd 127.0(2) . . ? C15 N5 Pd 114.7(2) . . ? C9 N6 C13 122.5(3) . . ? C9 N6 C12 125.4(3) . . ? C13 N6 C12 112.0(3) . . ? N1 C1 N3 121.9(4) . . ? N1 C1 N2 121.0(4) . . ? N3 C1 N2 117.0(4) . . ? N2 C2 C3 109.2(3) . . ? C4 C3 C2 107.6(4) . . ? N3 C4 C3 111.5(4) . . ? N3 C5 C6 112.6(4) . . ? C5 C6 C7 108.1(4) . . ? N1 C7 C6 109.5(3) . . ? N2 C8 N4 113.5(4) . . ? N5 C9 N6 123.1(3) . . ? N5 C9 N4 119.3(3) . . ? N6 C9 N4 117.6(3) . . ? N4 C10 C11 110.0(3) . . ? C12 C11 C10 108.4(4) . . ? N6 C12 C11 112.4(3) . . ? N6 C13 C14 111.6(3) . . ? C13 C14 C15 108.4(4) . . ? N5 C15 C14 110.1(3) . . ? #===END data_(2)-may1004 _database_code_depnum_ccdc_archive 'CCDC 743946' _audit_creation_date 2004-05-14T10:43:05-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C30 H52 Cl2 N12 Pd2, 2(C1 F3 O3 S1)' _chemical_formula_sum 'C32 H52 Cl2 F6 N12 O6 Pd2 S2' _chemical_formula_weight 1162.68 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.5796(2) _cell_length_b 10.6367(4) _cell_length_c 19.9015(6) _cell_angle_alpha 90 _cell_angle_beta 95.810(2) _cell_angle_gamma 90 _cell_volume 2228.05(12) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 39196 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.733 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.102 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8228 _exptl_absorpt_correction_T_max 0.9912 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.41039E-1 _diffrn_orient_matrix_ub_12 -0.243948E-1 _diffrn_orient_matrix_ub_13 -0.411936E-1 _diffrn_orient_matrix_ub_21 -0.833934E-1 _diffrn_orient_matrix_ub_22 -0.320726E-1 _diffrn_orient_matrix_ub_23 -0.213935E-1 _diffrn_orient_matrix_ub_31 -0.197021E-1 _diffrn_orient_matrix_ub_32 0.849405E-1 _diffrn_orient_matrix_ub_33 -0.199087E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.1015 _diffrn_reflns_av_unetI/netI 0.0439 _diffrn_reflns_number 31942 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.83 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 3921 _reflns_number_gt 3300 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The diffraction pattern suggested that the crystal was not single but it was possible to index many of the reflections as a rational cell. The structure solves and refines OK but there are a few residual peaks up to 3 electrons which make no chemical sense and are assumed to be spurious. The triflate anion is disordered and was refined with SADI constraints on equivalent dimensions and with the lower occupancy sites left isotropic. The C14 position was also disordered and the two sites left isotropic. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0709P)^2^+23.1169P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_number_reflns 3921 _refine_ls_number_parameters 305 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.0766 _refine_ls_R_factor_gt 0.0646 _refine_ls_wR_factor_ref 0.1763 _refine_ls_wR_factor_gt 0.1687 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.123 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.962 _refine_diff_density_min -0.779 _refine_diff_density_rms 0.156 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.06618(5) 0.11460(5) 0.05299(3) 0.0219(2) Uani 1 1 d . . . Cl Cl -0.11961(16) -0.00918(19) 0.04340(9) 0.0283(4) Uani 1 1 d . . . S S 0.3114(3) -0.3393(3) 0.17767(18) 0.0719(9) Uani 1 1 d D . . F1 F 0.1911(18) -0.3645(12) 0.0555(8) 0.160(10) Uani 0.759(17) 1 d PD . . F2 F 0.220(2) -0.1823(10) 0.0848(7) 0.151(9) Uani 0.759(17) 1 d PD . . F3 F 0.0870(12) -0.286(3) 0.1266(10) 0.215(12) Uani 0.759(17) 1 d PD . . O1 O 0.3182(15) -0.2398(13) 0.2233(6) 0.108(6) Uani 0.759(17) 1 d PD . . O2 O 0.4252(11) -0.3470(19) 0.1452(7) 0.135(8) Uani 0.759(17) 1 d PD . . O3 O 0.2695(19) -0.4529(14) 0.1974(11) 0.238(17) Uani 0.759(17) 1 d PD . . N1 N 0.0187(6) 0.2036(7) 0.1348(3) 0.0319(15) Uani 1 1 d . . . N2 N 0.2127(6) 0.1865(7) 0.2010(3) 0.0363(16) Uani 1 1 d . . . N3 N 0.0650(7) 0.3328(8) 0.2288(4) 0.0414(18) Uani 1 1 d . . . N4 N 0.3513(6) 0.0894(7) 0.1258(4) 0.0363(16) Uani 1 1 d . . . N5 N 0.2229(6) 0.2193(6) 0.0544(3) 0.0264(13) Uani 1 1 d . . . N6 N 0.4433(6) 0.2177(8) 0.0484(4) 0.048(2) Uani 1 1 d . . . C1 C 0.0976(7) 0.2404(8) 0.1871(4) 0.0325(18) Uani 1 1 d . . . C2 C -0.1099(7) 0.2592(9) 0.1285(5) 0.044(2) Uani 1 1 d . . . H2A H -0.1612 0.2208 0.1621 0.053 Uiso 1 1 calc R . . H2B H -0.1528 0.2428 0.0828 0.053 Uiso 1 1 calc R . . C3 C -0.0989(9) 0.3997(10) 0.1405(6) 0.055(3) Uani 1 1 d . . . H3A H -0.0452 0.4383 0.1081 0.065 Uiso 1 1 calc R . . H3B H -0.1839 0.4393 0.1344 0.065 Uiso 1 1 calc R . . C4 C -0.0393(10) 0.4187(11) 0.2120(6) 0.060(3) Uani 1 1 d . . . H4A H -0.008 0.5062 0.2174 0.072 Uiso 1 1 calc R . . H4B H -0.1045 0.406 0.2437 0.072 Uiso 1 1 calc R . . C5 C 0.1336(12) 0.3610(12) 0.2952(5) 0.064(3) Uani 1 1 d . . . H5A H 0.0736 0.3565 0.3302 0.077 Uiso 1 1 calc R . . H5B H 0.1673 0.4478 0.2948 0.077 Uiso 1 1 calc R . . C6 C 0.2396(12) 0.2729(12) 0.3129(5) 0.066(3) Uani 1 1 d . . . H6A H 0.2067 0.1938 0.3307 0.079 Uiso 1 1 calc R . . H6B H 0.3005 0.3103 0.3483 0.079 Uiso 1 1 calc R . . C7 C 0.3056(9) 0.2454(10) 0.2511(5) 0.048(2) Uani 1 1 d . . . H7A H 0.3381 0.3242 0.2328 0.058 Uiso 1 1 calc R . . H7B H 0.3783 0.188 0.2626 0.058 Uiso 1 1 calc R . . C8 C 0.2514(7) 0.0706(8) 0.1709(4) 0.0334(18) Uani 1 1 d . A . H8A H 0.1766 0.0317 0.1451 0.04 Uiso 1 1 calc R . . H8B H 0.2827 0.0115 0.2073 0.04 Uiso 1 1 calc R . . C9 C 0.3373(7) 0.1780(8) 0.0756(4) 0.0314(18) Uani 1 1 d . A . C10 C 0.2071(8) 0.3271(9) 0.0076(5) 0.039(2) Uani 1 1 d . A . H10A H 0.1421 0.3846 0.0228 0.047 Uiso 1 1 calc R . . H10B H 0.1756 0.2961 -0.0379 0.047 Uiso 1 1 calc R . . C11 C 0.3273(9) 0.3983(10) 0.0034(6) 0.054(3) Uani 1 1 d . . . H11A H 0.3169 0.4553 -0.0361 0.065 Uiso 1 1 calc R A . H11B H 0.3451 0.4505 0.0444 0.065 Uiso 1 1 calc R . . C12 C 0.4351(9) 0.3138(11) -0.0030(6) 0.056(3) Uani 1 1 d . A . H12A H 0.4253 0.2737 -0.0482 0.068 Uiso 1 1 calc R . . H12B H 0.5148 0.3632 0.0008 0.068 Uiso 1 1 calc R . . C16 C 0.2027(10) -0.2947(9) 0.1083(6) 0.070(3) Uani 1 1 d D . . F1A F 0.277(3) -0.277(3) 0.0618(15) 0.093(12) Uiso 0.241(17) 1 d PD . . F2A F 0.136(2) -0.197(2) 0.1110(14) 0.052(8) Uiso 0.241(17) 1 d PD . . F3A F 0.128(3) -0.385(3) 0.086(2) 0.098(15) Uiso 0.241(17) 1 d PD . . O1A O 0.389(3) -0.238(3) 0.196(3) 0.115(19) Uiso 0.241(17) 1 d PD . . O2A O 0.366(3) -0.4545(19) 0.1745(17) 0.066(11) Uiso 0.241(17) 1 d PD . . O3A O 0.202(3) -0.341(4) 0.214(3) 0.14(2) Uiso 0.241(17) 1 d PD . . C13 C 0.5710(9) 0.1788(14) 0.0746(8) 0.083(4) Uani 0.62(4) 1 d P A 1 H13A H 0.602 0.2311 0.114 0.1 Uiso 0.62(4) 1 calc PR A 1 H13B H 0.6301 0.1886 0.0395 0.1 Uiso 0.62(4) 1 calc PR A 1 C14 C 0.5635(16) 0.0384(18) 0.0959(10) 0.048(6) Uiso 0.62(4) 1 d P A 1 H14A H 0.5358 -0.0141 0.056 0.058 Uiso 0.62(4) 1 calc PR A 1 H14B H 0.6481 0.0088 0.1153 0.058 Uiso 0.62(4) 1 calc PR A 1 C15 C 0.4714(9) 0.0276(12) 0.1466(7) 0.066(3) Uani 0.62(4) 1 d P A 1 H15A H 0.4554 -0.0624 0.1549 0.079 Uiso 0.62(4) 1 calc PR A 1 H15B H 0.5088 0.0652 0.1896 0.079 Uiso 0.62(4) 1 calc PR A 1 C13A C 0.5710(9) 0.1788(14) 0.0746(8) 0.083(4) Uani 0.38(4) 1 d P A 2 H13C H 0.6137 0.1435 0.0369 0.1 Uiso 0.38(4) 1 calc PR A 2 H13D H 0.619 0.2546 0.0909 0.1 Uiso 0.38(4) 1 calc PR A 2 C14A C 0.579(3) 0.092(3) 0.1259(18) 0.055(10) Uiso 0.38(4) 1 d P A 2 H14C H 0.6194 0.1356 0.1665 0.065 Uiso 0.38(4) 1 calc PR A 2 H14D H 0.6391 0.027 0.1139 0.065 Uiso 0.38(4) 1 calc PR A 2 C15A C 0.4714(9) 0.0276(12) 0.1466(7) 0.066(3) Uani 0.38(4) 1 d P A 2 H15C H 0.4813 0.02 0.1964 0.079 Uiso 0.38(4) 1 calc PR A 2 H15D H 0.4693 -0.0584 0.1275 0.079 Uiso 0.38(4) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.0157(3) 0.0263(3) 0.0236(3) -0.0036(2) 0.0012(2) -0.0026(2) Cl 0.0215(8) 0.0383(11) 0.0258(9) -0.0057(8) 0.0059(7) -0.0072(8) S 0.0679(19) 0.0583(18) 0.086(2) 0.0179(17) -0.0094(16) 0.0014(15) F1 0.208(19) 0.083(10) 0.163(15) -0.079(10) -0.107(15) 0.076(11) F2 0.29(2) 0.051(7) 0.098(10) 0.020(7) -0.059(13) -0.008(10) F3 0.072(9) 0.34(3) 0.23(2) 0.06(2) 0.010(11) 0.095(15) O1 0.137(13) 0.130(13) 0.053(7) -0.027(8) -0.011(8) 0.057(11) O2 0.050(7) 0.26(2) 0.098(11) -0.030(13) 0.008(7) 0.008(11) O3 0.17(2) 0.131(18) 0.39(4) 0.19(2) -0.10(2) -0.061(15) N1 0.023(3) 0.039(4) 0.033(4) -0.013(3) 0.001(3) 0.000(3) N2 0.029(4) 0.042(4) 0.036(4) -0.008(3) -0.007(3) -0.001(3) N3 0.039(4) 0.051(5) 0.035(4) -0.016(3) 0.005(3) -0.008(4) N4 0.022(3) 0.038(4) 0.048(4) 0.011(3) 0.002(3) 0.002(3) N5 0.022(3) 0.026(3) 0.031(3) 0.000(3) 0.001(3) -0.002(3) N6 0.021(3) 0.052(5) 0.070(5) 0.016(4) 0.007(3) -0.007(3) C1 0.029(4) 0.038(5) 0.031(4) -0.012(4) 0.007(3) -0.009(4) C2 0.021(4) 0.056(6) 0.057(5) -0.021(5) 0.006(4) 0.003(4) C3 0.037(5) 0.051(6) 0.075(7) -0.019(5) -0.001(5) 0.014(4) C4 0.049(6) 0.058(7) 0.074(7) -0.038(6) 0.011(5) 0.003(5) C5 0.082(8) 0.074(8) 0.036(5) -0.023(5) 0.004(5) -0.016(7) C6 0.090(9) 0.069(8) 0.035(5) -0.007(5) -0.013(5) -0.029(7) C7 0.044(5) 0.049(6) 0.048(5) -0.007(5) -0.017(4) -0.016(5) C8 0.028(4) 0.038(5) 0.034(4) 0.010(4) -0.003(3) -0.006(4) C9 0.022(4) 0.029(4) 0.043(5) -0.002(4) 0.003(3) -0.004(3) C10 0.028(4) 0.035(5) 0.052(5) 0.013(4) -0.003(4) 0.001(4) C11 0.043(5) 0.048(6) 0.071(7) 0.024(5) 0.009(5) -0.007(5) C12 0.036(5) 0.061(7) 0.073(7) 0.023(6) 0.006(5) -0.008(5) C16 0.064(7) 0.049(7) 0.095(9) -0.016(7) -0.007(7) 0.015(6) C13 0.021(5) 0.085(9) 0.144(13) 0.044(9) 0.009(6) 0.001(5) C15 0.031(5) 0.059(7) 0.107(10) 0.029(7) 0.006(5) 0.008(5) C13A 0.021(5) 0.085(9) 0.144(13) 0.044(9) 0.009(6) 0.001(5) C15A 0.031(5) 0.059(7) 0.107(10) 0.029(7) 0.006(5) 0.008(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd N1 1.991(6) . ? Pd N5 1.995(6) . ? Pd Cl 2.3402(18) 3 ? Pd Cl 2.3573(18) . ? S O3 1.359(11) . ? S O2A 1.359(15) . ? S O1A 1.380(15) . ? S O1 1.392(11) . ? S O2 1.425(11) . ? S O3A 1.425(16) . ? S C16 1.770(13) . ? F1 C16 1.281(12) . ? F2 C16 1.303(12) . ? F3 F2A 1.14(3) . ? F3 C16 1.314(12) . ? N1 C1 1.326(10) . ? N1 C2 1.477(10) . ? N2 C1 1.350(11) . ? N2 C8 1.447(11) . ? N2 C7 1.468(10) . ? N3 C1 1.353(11) . ? N3 C4 1.446(14) . ? N3 C5 1.472(12) . ? N4 C9 1.371(11) . ? N4 C15 1.453(12) . ? N4 C8 1.469(10) . ? N5 C9 1.315(10) . ? N5 C10 1.476(10) . ? N6 C9 1.360(10) . ? N6 C12 1.443(13) . ? N6 C13 1.458(12) . ? C2 C3 1.516(14) . ? C3 C4 1.511(15) . ? C5 C6 1.476(17) . ? C6 C7 1.503(15) . ? C10 C11 1.490(12) . ? C11 C12 1.468(15) . ? C16 F2A 1.262(15) . ? C16 F1A 1.285(15) . ? C16 F3A 1.288(16) . ? C13 C14 1.56(2) . ? C14 C15 1.48(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd N5 90.1(3) . . ? N1 Pd Cl 179.34(19) . 3 ? N5 Pd Cl 90.56(19) . 3 ? N1 Pd Cl 93.11(19) . . ? N5 Pd Cl 176.20(18) . . ? Cl Pd Cl 86.25(6) 3 . ? Pd Cl Pd 93.75(6) 3 . ? O2A S O1A 118.1(14) . . ? O3 S O1 118.9(10) . . ? O3 S O2 113.3(10) . . ? O1 S O2 110.5(8) . . ? O2A S O3A 112.5(14) . . ? O1A S O3A 111.6(14) . . ? O3 S C16 105.0(9) . . ? O2A S C16 116.8(15) . . ? O1A S C16 109(2) . . ? O1 S C16 107.0(6) . . ? O2 S C16 100.0(8) . . ? O3A S C16 84(2) . . ? C1 N1 C2 116.7(7) . . ? C1 N1 Pd 126.3(5) . . ? C2 N1 Pd 115.3(5) . . ? C1 N2 C8 124.4(6) . . ? C1 N2 C7 119.1(7) . . ? C8 N2 C7 116.5(7) . . ? C1 N3 C4 123.6(7) . . ? C1 N3 C5 124.4(9) . . ? C4 N3 C5 112.0(8) . . ? C9 N4 C15 123.1(7) . . ? C9 N4 C8 120.6(7) . . ? C15 N4 C8 115.2(7) . . ? C9 N5 C10 120.2(6) . . ? C9 N5 Pd 123.7(5) . . ? C10 N5 Pd 112.5(5) . . ? C9 N6 C12 120.6(7) . . ? C9 N6 C13 122.7(8) . . ? C12 N6 C13 116.2(8) . . ? N1 C1 N2 121.2(7) . . ? N1 C1 N3 121.1(7) . . ? N2 C1 N3 117.7(7) . . ? N1 C2 C3 109.0(7) . . ? C4 C3 C2 107.4(9) . . ? N3 C4 C3 111.7(8) . . ? N3 C5 C6 112.2(9) . . ? C5 C6 C7 109.5(9) . . ? N2 C7 C6 107.7(8) . . ? N2 C8 N4 112.8(7) . . ? N5 C9 N6 122.6(8) . . ? N5 C9 N4 119.3(7) . . ? N6 C9 N4 118.1(7) . . ? N5 C10 C11 112.8(7) . . ? C12 C11 C10 111.7(9) . . ? N6 C12 C11 111.3(9) . . ? F2A C16 F1A 107.1(15) . . ? F2A C16 F3A 107.6(16) . . ? F1A C16 F3A 104.9(15) . . ? F1 C16 F2 104.1(11) . . ? F1 C16 F3 104.5(12) . . ? F2 C16 F3 102.0(11) . . ? F2A C16 S 120.7(15) . . ? F1 C16 S 119.0(9) . . ? F1A C16 S 101.9(17) . . ? F3A C16 S 113(2) . . ? F2 C16 S 114.9(10) . . ? F3 C16 S 110.5(11) . . ? N6 C13 C14 107.4(10) . . ? C15 C14 C13 108.4(14) . . ? N4 C15 C14 112.9(11) . . ? #===END data_(3)-jan608 _database_code_depnum_ccdc_archive 'CCDC 743947' _audit_creation_date 2008-01-10T15:49:03-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C11 H18 N6' _chemical_formula_sum 'C11 H18 N6' _chemical_formula_weight 234.31 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.4850(2) _cell_length_b 10.3589(5) _cell_length_c 10.7342(5) _cell_angle_alpha 75.157(2) _cell_angle_beta 83.025(3) _cell_angle_gamma 84.728(3) _cell_volume 584.01(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5915 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.332 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 252 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.087 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.19515E-1 _diffrn_orient_matrix_ub_12 -0.80073E-2 _diffrn_orient_matrix_ub_13 0.954709E-1 _diffrn_orient_matrix_ub_21 0.182885 _diffrn_orient_matrix_ub_22 -0.35931E-2 _diffrn_orient_matrix_ub_23 -0.3286E-3 _diffrn_orient_matrix_ub_31 -0.66792E-2 _diffrn_orient_matrix_ub_32 0.996832E-1 _diffrn_orient_matrix_ub_33 -0.164509E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0729 _diffrn_reflns_av_unetI/netI 0.049 _diffrn_reflns_number 8249 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.75 _diffrn_reflns_theta_max 25.89 _diffrn_reflns_theta_full 25.89 _diffrn_measured_fraction_theta_full 0.969 _diffrn_measured_fraction_theta_max 0.969 _reflns_number_total 2195 _reflns_number_gt 1808 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0601P)^2^+0.1392P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 2195 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0564 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.12 _refine_ls_wR_factor_gt 0.1116 _refine_ls_goodness_of_fit_ref 1.01 _refine_ls_restrained_S_all 1.01 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.197 _refine_diff_density_min -0.21 _refine_diff_density_rms 0.041 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.1576(2) 0.43692(12) 0.86409(12) 0.0306(3) Uani 1 1 d . . . N2 N -0.1061(2) 0.36995(12) 0.72945(13) 0.0341(3) Uani 1 1 d . . . N3 N 0.1732(2) 0.22428(12) 0.84723(12) 0.0302(3) Uani 1 1 d . . . N4 N 0.3424(2) 0.63187(12) 0.72766(12) 0.0327(3) Uani 1 1 d . . . N5 N 0.3934(3) 0.83463(13) 0.79144(13) 0.0411(4) Uani 1 1 d . . . N6 N 0.5476(2) 0.79856(12) 0.59282(12) 0.0324(3) Uani 1 1 d . . . C1 C 0.0652(2) 0.35228(14) 0.80512(14) 0.0273(3) Uani 1 1 d . . . C2 C 0.3495(3) 0.36307(16) 0.94390(15) 0.0340(4) Uani 1 1 d . . . H2A H 0.3433 0.3903 1.0262 0.041 Uiso 1 1 calc R . . H2B H 0.5158 0.3757 0.8968 0.041 Uiso 1 1 calc R . . C3 C 0.2782(3) 0.21872(16) 0.96731(16) 0.0351(4) Uani 1 1 d . . . H3A H 0.4237 0.1545 0.9789 0.042 Uiso 1 1 calc R . . H3B H 0.1554 0.1945 1.0437 0.042 Uiso 1 1 calc R . . C4 C -0.0144(3) 0.13775(16) 0.83408(17) 0.0374(4) Uani 1 1 d . . . H4A H -0.1298 0.1143 0.9137 0.045 Uiso 1 1 calc R . . H4B H 0.0601 0.055 0.8114 0.045 Uiso 1 1 calc R . . C5 C -0.1401(3) 0.23230(16) 0.72094(17) 0.0382(4) Uani 1 1 d . . . H5A H -0.0629 0.2177 0.637 0.046 Uiso 1 1 calc R . . H5B H -0.3174 0.2166 0.7292 0.046 Uiso 1 1 calc R . . C6 C 0.1353(3) 0.57984(14) 0.81826(15) 0.0319(4) Uani 1 1 d . . . H6A H 0.1224 0.6204 0.8931 0.038 Uiso 1 1 calc R . . H6B H -0.018 0.6062 0.7755 0.038 Uiso 1 1 calc R . . C7 C 0.4158(3) 0.75724(14) 0.71326(14) 0.0301(4) Uani 1 1 d . . . C8 C 0.4130(3) 0.58928(15) 0.60783(15) 0.0321(4) Uani 1 1 d . . . H8A H 0.2749 0.6049 0.5532 0.039 Uiso 1 1 calc R . . H8B H 0.4709 0.4936 0.6258 0.039 Uiso 1 1 calc R . . C9 C 0.6229(3) 0.68015(15) 0.54406(16) 0.0346(4) Uani 1 1 d . . . H9A H 0.7838 0.6393 0.5722 0.042 Uiso 1 1 calc R . . H9B H 0.6317 0.7013 0.4484 0.042 Uiso 1 1 calc R . . C10 C 0.7066(3) 0.89692(17) 0.61104(18) 0.0435(5) Uani 1 1 d . . . H10A H 0.7357 0.9694 0.5314 0.052 Uiso 1 1 calc R . . H10B H 0.8663 0.8548 0.6399 0.052 Uiso 1 1 calc R . . C11 C 0.5450(4) 0.94759(17) 0.71868(18) 0.0479(5) Uani 1 1 d . . . H11A H 0.6488 0.9729 0.7768 0.058 Uiso 1 1 calc R . . H11B H 0.438 1.0267 0.6808 0.058 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0336(7) 0.0238(7) 0.0322(7) -0.0018(5) -0.0023(5) -0.0070(5) N2 0.0310(7) 0.0279(7) 0.0413(8) -0.0020(6) -0.0051(6) -0.0086(5) N3 0.0262(6) 0.0243(7) 0.0379(8) -0.0033(5) -0.0021(5) -0.0043(5) N4 0.0420(7) 0.0234(7) 0.0325(7) -0.0083(6) 0.0075(6) -0.0118(5) N5 0.0612(9) 0.0258(7) 0.0381(8) -0.0062(6) -0.0078(7) -0.0133(6) N6 0.0342(7) 0.0262(7) 0.0342(7) 0.0002(6) -0.0033(6) -0.0105(5) C1 0.0252(7) 0.0242(8) 0.0289(8) -0.0019(6) 0.0047(6) -0.0068(6) C2 0.0317(8) 0.0369(9) 0.0319(8) -0.0047(7) -0.0020(6) -0.0071(6) C3 0.0311(8) 0.0336(9) 0.0365(9) -0.0016(7) -0.0033(7) -0.0007(6) C4 0.0326(8) 0.0264(8) 0.0516(11) -0.0054(7) -0.0026(7) -0.0079(6) C5 0.0338(8) 0.0325(9) 0.0487(10) -0.0073(8) -0.0054(7) -0.0100(7) C6 0.0365(8) 0.0250(8) 0.0325(8) -0.0061(6) 0.0048(6) -0.0065(6) C7 0.0353(8) 0.0229(8) 0.0304(8) -0.0010(6) -0.0065(6) -0.0046(6) C8 0.0369(8) 0.0283(8) 0.0307(8) -0.0083(6) 0.0026(7) -0.0058(6) C9 0.0338(8) 0.0318(9) 0.0344(9) -0.0032(7) 0.0022(7) -0.0044(6) C10 0.0445(10) 0.0321(9) 0.0502(11) 0.0063(8) -0.0156(8) -0.0157(7) C11 0.0717(12) 0.0285(9) 0.0444(11) 0.0005(8) -0.0186(9) -0.0179(8) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C1 1.3676(19) . ? N1 C6 1.4343(19) . ? N1 C2 1.4705(19) . ? N2 C1 1.2861(19) . ? N2 C5 1.482(2) . ? N3 C1 1.3881(19) . ? N3 C3 1.460(2) . ? N3 C4 1.4669(19) . ? N4 C7 1.3604(18) . ? N4 C6 1.4499(19) . ? N4 C8 1.462(2) . ? N5 C7 1.290(2) . ? N5 C11 1.491(2) . ? N6 C7 1.387(2) . ? N6 C9 1.460(2) . ? N6 C10 1.4642(19) . ? C2 C3 1.531(2) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? C4 C5 1.543(2) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? C8 C9 1.536(2) . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? C9 H9A 0.99 . ? C9 H9B 0.99 . ? C10 C11 1.540(3) . ? C10 H10A 0.99 . ? C10 H10B 0.99 . ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 C6 123.19(13) . . ? C1 N1 C2 109.05(12) . . ? C6 N1 C2 124.20(12) . . ? C1 N2 C5 103.03(12) . . ? C1 N3 C3 107.42(12) . . ? C1 N3 C4 103.32(11) . . ? C3 N3 C4 125.03(13) . . ? C7 N4 C6 122.14(13) . . ? C7 N4 C8 109.65(12) . . ? C6 N4 C8 122.38(12) . . ? C7 N5 C11 102.50(14) . . ? C7 N6 C9 107.92(12) . . ? C7 N6 C10 103.67(13) . . ? C9 N6 C10 127.28(13) . . ? N2 C1 N1 131.79(14) . . ? N2 C1 N3 118.62(13) . . ? N1 C1 N3 109.39(13) . . ? N1 C2 C3 101.38(11) . . ? N1 C2 H2A 111.5 . . ? C3 C2 H2A 111.5 . . ? N1 C2 H2B 111.5 . . ? C3 C2 H2B 111.5 . . ? H2A C2 H2B 109.3 . . ? N3 C3 C2 101.18(12) . . ? N3 C3 H3A 111.5 . . ? C2 C3 H3A 111.5 . . ? N3 C3 H3B 111.5 . . ? C2 C3 H3B 111.5 . . ? H3A C3 H3B 109.4 . . ? N3 C4 C5 99.52(12) . . ? N3 C4 H4A 111.9 . . ? C5 C4 H4A 111.9 . . ? N3 C4 H4B 111.9 . . ? C5 C4 H4B 111.9 . . ? H4A C4 H4B 109.6 . . ? N2 C5 C4 105.93(13) . . ? N2 C5 H5A 110.5 . . ? C4 C5 H5A 110.5 . . ? N2 C5 H5B 110.5 . . ? C4 C5 H5B 110.5 . . ? H5A C5 H5B 108.7 . . ? N1 C6 N4 112.49(12) . . ? N1 C6 H6A 109.1 . . ? N4 C6 H6A 109.1 . . ? N1 C6 H6B 109.1 . . ? N4 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? N5 C7 N4 131.72(14) . . ? N5 C7 N6 118.83(13) . . ? N4 C7 N6 109.35(13) . . ? N4 C8 C9 101.64(12) . . ? N4 C8 H8A 111.4 . . ? C9 C8 H8A 111.4 . . ? N4 C8 H8B 111.4 . . ? C9 C8 H8B 111.4 . . ? H8A C8 H8B 109.3 . . ? N6 C9 C8 101.14(12) . . ? N6 C9 H9A 111.5 . . ? C8 C9 H9A 111.5 . . ? N6 C9 H9B 111.5 . . ? C8 C9 H9B 111.5 . . ? H9A C9 H9B 109.4 . . ? N6 C10 C11 99.59(13) . . ? N6 C10 H10A 111.9 . . ? C11 C10 H10A 111.9 . . ? N6 C10 H10B 111.9 . . ? C11 C10 H10B 111.9 . . ? H10A C10 H10B 109.6 . . ? N5 C11 C10 106.14(13) . . ? N5 C11 H11A 110.5 . . ? C10 C11 H11A 110.5 . . ? N5 C11 H11B 110.5 . . ? C10 C11 H11B 110.5 . . ? H11A C11 H11B 108.7 . . ? #===END data_(3H2O)-nov707 _database_code_depnum_ccdc_archive 'CCDC 743948' _audit_creation_date 2007-11-16T11:08:35-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C11 H18 N6, H2 O' _chemical_formula_sum 'C11 H20 N6 O' _chemical_formula_weight 252.33 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.2368(4) _cell_length_b 12.4194(8) _cell_length_c 13.7735(11) _cell_angle_alpha 90 _cell_angle_beta 95.158(4) _cell_angle_gamma 90 _cell_volume 1232.90(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9688 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.359 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 544 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.094 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.780122E-1 _diffrn_orient_matrix_ub_12 0.115966E-1 _diffrn_orient_matrix_ub_13 -0.62807E-1 _diffrn_orient_matrix_ub_21 0.982972E-1 _diffrn_orient_matrix_ub_22 -0.341387E-1 _diffrn_orient_matrix_ub_23 -0.363179E-1 _diffrn_orient_matrix_ub_31 -0.591759E-1 _diffrn_orient_matrix_ub_32 -0.719959E-1 _diffrn_orient_matrix_ub_33 0.71045E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0703 _diffrn_reflns_av_unetI/netI 0.0613 _diffrn_reflns_number 9754 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.48 _diffrn_reflns_theta_max 25.99 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 2397 _reflns_number_gt 1619 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The watrer H atoms were refined. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0467P)^2^+0.4593P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 2397 _refine_ls_number_parameters 171 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0922 _refine_ls_R_factor_gt 0.0528 _refine_ls_wR_factor_ref 0.1193 _refine_ls_wR_factor_gt 0.1047 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.155 _refine_diff_density_min -0.222 _refine_diff_density_rms 0.046 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.0819(2) 0.16982(14) 0.28070(13) 0.0327(4) Uani 1 1 d . . . N2 N -0.2426(2) 0.16200(14) 0.21950(13) 0.0322(4) Uani 1 1 d . . . N3 N -0.0221(2) 0.04499(13) 0.17162(12) 0.0291(4) Uani 1 1 d . . . N4 N 0.0864(2) 0.22237(13) 0.45149(12) 0.0281(4) Uani 1 1 d . . . N5 N 0.4159(2) 0.19906(13) 0.49832(13) 0.0313(4) Uani 1 1 d . . . N6 N 0.1922(2) 0.10009(13) 0.56449(12) 0.0277(4) Uani 1 1 d . . . C1 C -0.0723(3) 0.13081(15) 0.22835(15) 0.0274(5) Uani 1 1 d . . . C2 C 0.2451(3) 0.10852(17) 0.25764(16) 0.0329(5) Uani 1 1 d . . . H2A H 0.2796 0.0535 0.308 0.039 Uiso 1 1 calc R . . H2B H 0.3526 0.1564 0.2508 0.039 Uiso 1 1 calc R . . C3 C 0.1767(3) 0.05653(17) 0.16015(16) 0.0339(5) Uani 1 1 d . . . H3A H 0.1986 0.1038 0.1044 0.041 Uiso 1 1 calc R . . H3B H 0.2363 -0.0142 0.1516 0.041 Uiso 1 1 calc R . . C4 C -0.1678(3) 0.04314(17) 0.09060(16) 0.0330(5) Uani 1 1 d . . . H4A H -0.1948 -0.0311 0.0672 0.04 Uiso 1 1 calc R . . H4B H -0.1353 0.0885 0.0355 0.04 Uiso 1 1 calc R . . C5 C -0.3304(3) 0.09099(17) 0.14099(16) 0.0336(5) Uani 1 1 d . . . H5A H -0.4133 0.1331 0.0942 0.04 Uiso 1 1 calc R . . H5B H -0.4035 0.0333 0.169 0.04 Uiso 1 1 calc R . . C6 C 0.0855(3) 0.25659(16) 0.35107(15) 0.0293(5) Uani 1 1 d . . . H6A H 0.1973 0.301 0.3444 0.035 Uiso 1 1 calc R . . H6B H -0.0243 0.303 0.3351 0.035 Uiso 1 1 calc R . . C7 C 0.2427(3) 0.17735(15) 0.50013(15) 0.0255(5) Uani 1 1 d . . . C8 C -0.0772(3) 0.16687(17) 0.48438(16) 0.0301(5) Uani 1 1 d . . . H8A H -0.1222 0.1098 0.4379 0.036 Uiso 1 1 calc R . . H8B H -0.1794 0.2182 0.4925 0.036 Uiso 1 1 calc R . . C9 C -0.0013(3) 0.11892(17) 0.58248(16) 0.0319(5) Uani 1 1 d . . . H9A H -0.0116 0.1703 0.6367 0.038 Uiso 1 1 calc R . . H9B H -0.0652 0.051 0.5967 0.038 Uiso 1 1 calc R . . C10 C 0.3505(3) 0.09071(18) 0.63719(16) 0.0331(5) Uani 1 1 d . . . H10A H 0.3701 0.0154 0.6594 0.04 Uiso 1 1 calc R . . H10B H 0.337 0.1377 0.6942 0.04 Uiso 1 1 calc R . . C11 C 0.5074(3) 0.12969(17) 0.57697(16) 0.0331(5) Uani 1 1 d . . . H11A H 0.6008 0.1714 0.6184 0.04 Uiso 1 1 calc R . . H11B H 0.5699 0.0677 0.5487 0.04 Uiso 1 1 calc R . . O O 0.5844(2) 0.31606(13) 0.34554(14) 0.0425(4) Uani 1 1 d . . . H2X H 0.639(5) 0.264(3) 0.309(3) 0.098(12) Uiso 1 1 d . . . H1X H 0.539(5) 0.276(3) 0.399(3) 0.094(11) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0256(9) 0.0389(10) 0.0328(11) -0.0086(9) -0.0013(7) 0.0034(8) N2 0.0278(10) 0.0364(10) 0.0316(11) -0.0015(8) -0.0009(7) 0.0022(8) N3 0.0277(9) 0.0290(9) 0.0303(11) -0.0023(8) 0.0014(8) 0.0028(7) N4 0.0249(9) 0.0316(9) 0.0276(11) -0.0010(8) 0.0016(7) -0.0023(7) N5 0.0252(9) 0.0369(10) 0.0311(11) -0.0007(8) -0.0021(8) -0.0026(8) N6 0.0228(9) 0.0315(9) 0.0286(10) 0.0011(8) 0.0011(7) -0.0007(7) C1 0.0277(11) 0.0285(11) 0.0261(12) 0.0013(9) 0.0026(9) -0.0002(9) C2 0.0257(11) 0.0359(12) 0.0369(14) -0.0002(10) 0.0023(9) 0.0032(9) C3 0.0291(12) 0.0342(12) 0.0388(14) -0.0035(10) 0.0059(10) 0.0037(9) C4 0.0360(12) 0.0304(12) 0.0316(14) -0.0025(10) -0.0020(10) -0.0007(9) C5 0.0298(12) 0.0366(12) 0.0330(14) -0.0010(10) -0.0047(9) -0.0009(9) C6 0.0306(11) 0.0279(11) 0.0288(13) 0.0007(9) 0.0004(9) -0.0002(9) C7 0.0258(11) 0.0251(10) 0.0256(12) -0.0036(9) 0.0020(8) -0.0002(8) C8 0.0223(10) 0.0326(11) 0.0355(13) -0.0009(10) 0.0024(9) 0.0000(8) C9 0.0276(11) 0.0352(12) 0.0333(13) -0.0014(10) 0.0062(9) -0.0007(9) C10 0.0280(11) 0.0386(12) 0.0314(13) 0.0013(10) -0.0036(9) -0.0009(9) C11 0.0269(11) 0.0363(12) 0.0350(14) -0.0016(10) -0.0029(9) -0.0014(9) O 0.0419(10) 0.0369(9) 0.0493(12) 0.0042(9) 0.0065(8) 0.0003(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C1 1.362(3) . ? N1 C6 1.448(3) . ? N1 C2 1.464(3) . ? N2 C1 1.287(2) . ? N2 C5 1.492(3) . ? N3 C1 1.389(3) . ? N3 C4 1.465(3) . ? N3 C3 1.468(2) . ? N4 C7 1.380(3) . ? N4 C6 1.446(3) . ? N4 C8 1.476(2) . ? N5 C7 1.284(2) . ? N5 C11 1.492(3) . ? N6 C7 1.378(3) . ? N6 C10 1.457(3) . ? N6 C9 1.463(2) . ? C2 C3 1.532(3) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? C4 C5 1.538(3) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? C8 C9 1.532(3) . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? C9 H9A 0.99 . ? C9 H9B 0.99 . ? C10 C11 1.543(3) . ? C10 H10A 0.99 . ? C10 H10B 0.99 . ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? O H2X 0.93(4) . ? O H1X 0.97(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 C6 125.72(16) . . ? C1 N1 C2 109.80(16) . . ? C6 N1 C2 124.46(16) . . ? C1 N2 C5 103.44(16) . . ? C1 N3 C4 103.53(15) . . ? C1 N3 C3 107.09(15) . . ? C4 N3 C3 124.38(17) . . ? C7 N4 C6 121.08(16) . . ? C7 N4 C8 107.88(16) . . ? C6 N4 C8 119.73(16) . . ? C7 N5 C11 103.60(16) . . ? C7 N6 C10 105.08(16) . . ? C7 N6 C9 108.13(15) . . ? C10 N6 C9 127.01(17) . . ? N2 C1 N1 132.45(19) . . ? N2 C1 N3 118.30(18) . . ? N1 C1 N3 109.13(16) . . ? N1 C2 C3 101.88(16) . . ? N1 C2 H2A 111.4 . . ? C3 C2 H2A 111.4 . . ? N1 C2 H2B 111.4 . . ? C3 C2 H2B 111.4 . . ? H2A C2 H2B 109.3 . . ? N3 C3 C2 100.92(16) . . ? N3 C3 H3A 111.6 . . ? C2 C3 H3A 111.6 . . ? N3 C3 H3B 111.6 . . ? C2 C3 H3B 111.6 . . ? H3A C3 H3B 109.4 . . ? N3 C4 C5 100.22(16) . . ? N3 C4 H4A 111.7 . . ? C5 C4 H4A 111.7 . . ? N3 C4 H4B 111.7 . . ? C5 C4 H4B 111.7 . . ? H4A C4 H4B 109.5 . . ? N2 C5 C4 105.21(16) . . ? N2 C5 H5A 110.7 . . ? C4 C5 H5A 110.7 . . ? N2 C5 H5B 110.7 . . ? C4 C5 H5B 110.7 . . ? H5A C5 H5B 108.8 . . ? N4 C6 N1 114.81(16) . . ? N4 C6 H6A 108.6 . . ? N1 C6 H6A 108.6 . . ? N4 C6 H6B 108.6 . . ? N1 C6 H6B 108.6 . . ? H6A C6 H6B 107.5 . . ? N5 C7 N6 118.33(18) . . ? N5 C7 N4 131.62(19) . . ? N6 C7 N4 109.94(16) . . ? N4 C8 C9 102.60(15) . . ? N4 C8 H8A 111.2 . . ? C9 C8 H8A 111.2 . . ? N4 C8 H8B 111.2 . . ? C9 C8 H8B 111.2 . . ? H8A C8 H8B 109.2 . . ? N6 C9 C8 100.70(16) . . ? N6 C9 H9A 111.6 . . ? C8 C9 H9A 111.6 . . ? N6 C9 H9B 111.6 . . ? C8 C9 H9B 111.6 . . ? H9A C9 H9B 109.4 . . ? N6 C10 C11 100.18(16) . . ? N6 C10 H10A 111.7 . . ? C11 C10 H10A 111.7 . . ? N6 C10 H10B 111.7 . . ? C11 C10 H10B 111.7 . . ? H10A C10 H10B 109.5 . . ? N5 C11 C10 105.73(16) . . ? N5 C11 H11A 110.6 . . ? C10 C11 H11A 110.6 . . ? N5 C11 H11B 110.6 . . ? C10 C11 H11B 110.6 . . ? H11A C11 H11B 108.7 . . ? H2X O H1X 105(3) . . ? #===END data_(4)-may808 _database_code_depnum_ccdc_archive 'CCDC 743949' _audit_creation_date 2008-05-19T07:32:45-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C22 H36 N12 Pd, 5(C H2 Cl2), 2(Cl)' _chemical_formula_sum 'C27 H46 Cl12 N12 Pd' _chemical_formula_weight 1070.58 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 11.2121(3) _cell_length_b 17.9696(7) _cell_length_c 22.7166(8) _cell_angle_alpha 90 _cell_angle_beta 96.199(2) _cell_angle_gamma 90 _cell_volume 4550.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 12314 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2168 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.149 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.6771 _exptl_absorpt_correction_T_max 0.7981 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.50733E-1 _diffrn_orient_matrix_ub_12 -0.356219E-1 _diffrn_orient_matrix_ub_13 -0.201899E-1 _diffrn_orient_matrix_ub_21 0.617413E-1 _diffrn_orient_matrix_ub_22 0.10418E-2 _diffrn_orient_matrix_ub_23 0.352176E-1 _diffrn_orient_matrix_ub_31 -0.407769E-1 _diffrn_orient_matrix_ub_32 -0.427418E-1 _diffrn_orient_matrix_ub_33 0.176851E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0787 _diffrn_reflns_av_unetI/netI 0.0627 _diffrn_reflns_number 16915 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 26.14 _diffrn_reflns_theta_full 26.14 _diffrn_measured_fraction_theta_full 0.977 _diffrn_measured_fraction_theta_max 0.977 _reflns_number_total 4430 _reflns_number_gt 3256 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Nitrogen N3 was disordered over two resolved positions. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0689P)^2^+10.3903P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 4430 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0791 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1452 _refine_ls_wR_factor_gt 0.1223 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.966 _refine_diff_density_min -1.043 _refine_diff_density_rms 0.253 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.25 0.25 0.5 0.02494(17) Uani 1 2 d S . . Cl1 Cl 0.25860(10) 0.02406(7) 0.25903(5) 0.0365(3) Uani 1 1 d . . . N1 N 0.2837(3) 0.3087(2) 0.42827(14) 0.0295(8) Uani 1 1 d . C . N2 N 0.2601(3) 0.2238(2) 0.34492(15) 0.0296(8) Uani 1 1 d . C . N4 N 0.0986(3) 0.1508(2) 0.37849(15) 0.0312(8) Uani 1 1 d . C . N5 N 0.0814(3) 0.2263(2) 0.46513(14) 0.0295(8) Uani 1 1 d . . . N6 N -0.0790(3) 0.1863(2) 0.40526(15) 0.0334(9) Uani 1 1 d . . . C1 C 0.2795(4) 0.2887(3) 0.37299(18) 0.0315(10) Uani 1 1 d . . . C2 C 0.3148(6) 0.3890(3) 0.4300(2) 0.0507(14) Uani 1 1 d . . . H2B H 0.3847 0.3987 0.4595 0.061 Uiso 1 1 calc R A 1 H2A H 0.2462 0.4194 0.44 0.061 Uiso 1 1 calc R A 1 C5 C 0.2662(5) 0.2352(3) 0.28100(19) 0.0414(13) Uani 1 1 d . . . H5B H 0.1854 0.233 0.2587 0.05 Uiso 1 1 calc R B 1 H5A H 0.3184 0.1976 0.2649 0.05 Uiso 1 1 calc R B 1 C6 C 0.0432(4) 0.1903(2) 0.41750(17) 0.0271(9) Uani 1 1 d . . . C7 C -0.0279(4) 0.2506(3) 0.4916(2) 0.0423(12) Uani 1 1 d . . . H7B H -0.0452 0.3038 0.4831 0.051 Uiso 1 1 calc R . . H7A H -0.0185 0.243 0.535 0.051 Uiso 1 1 calc R . . C8 C -0.1271(4) 0.2009(3) 0.4615(2) 0.0453(13) Uani 1 1 d . . . H8B H -0.1362 0.1546 0.4841 0.054 Uiso 1 1 calc R . . H8A H -0.205 0.2273 0.4556 0.054 Uiso 1 1 calc R . . C9 C -0.1054(4) 0.1215(3) 0.3672(2) 0.0454(13) Uani 1 1 d . . . H9B H -0.1796 0.1286 0.34 0.054 Uiso 1 1 calc R . . H9A H -0.1126 0.0756 0.3907 0.054 Uiso 1 1 calc R . . C10 C 0.0064(4) 0.1197(3) 0.3337(2) 0.0434(12) Uani 1 1 d . . . H10B H 0.0265 0.0684 0.3226 0.052 Uiso 1 1 calc R . . H10A H -0.0042 0.1511 0.2977 0.052 Uiso 1 1 calc R . . C11 C 0.2248(4) 0.1560(2) 0.37168(18) 0.0278(9) Uani 1 1 d . . . H11B H 0.2709 0.1511 0.4112 0.033 Uiso 1 1 calc R C . H11A H 0.247 0.1136 0.3473 0.033 Uiso 1 1 calc R . . Cl1S Cl 0.56070(15) 0.17055(10) 0.34689(8) 0.0721(5) Uani 1 1 d . . . Cl2S Cl 0.5459(3) 0.03728(15) 0.41688(11) 0.1163(8) Uani 1 1 d . . . Cl3S Cl 0.17891(18) -0.15819(10) 0.38251(7) 0.0764(5) Uani 1 1 d . . . Cl4S Cl 0.1844(3) -0.01769(11) 0.44287(9) 0.1071(8) Uani 1 1 d . . . Cl5S Cl 0.51796(14) 0.16160(10) 0.68722(7) 0.0665(5) Uani 1 1 d . . . C1S C 0.5404(5) 0.0727(4) 0.3454(3) 0.0647(18) Uani 1 1 d . . . H1S2 H 0.4619 0.0605 0.3232 0.078 Uiso 1 1 calc R . . H1S1 H 0.6039 0.0492 0.3246 0.078 Uiso 1 1 calc R . . C2S C 0.2513(6) -0.0732(3) 0.3928(3) 0.0653(17) Uani 1 1 d . . . H2S2 H 0.2489 -0.047 0.3544 0.078 Uiso 1 1 calc R . . H2S1 H 0.3365 -0.0816 0.4078 0.078 Uiso 1 1 calc R . . C3S C 0.5 0.1057(5) 0.75 0.063(2) Uani 1 2 d S . . H3S2 H 0.4288 0.0733 0.7414 0.076 Uiso 0.5 1 calc PR . . H3S1 H 0.5712 0.0733 0.7586 0.076 Uiso 0.5 1 calc PR . . C3 C 0.3450(5) 0.4067(3) 0.3672(2) 0.0436(12) Uani 0.65(4) 1 d P C 1 H3A H 0.3127 0.4557 0.3534 0.052 Uiso 0.65(4) 1 calc PR C 1 H3B H 0.4326 0.4056 0.3648 0.052 Uiso 0.65(4) 1 calc PR C 1 C4 C 0.3201(4) 0.3133(3) 0.2786(2) 0.0413(12) Uani 0.65(4) 1 d P C 1 H4A H 0.4084 0.3115 0.2789 0.05 Uiso 0.65(4) 1 calc PR C 1 H4B H 0.285 0.3411 0.2432 0.05 Uiso 0.65(4) 1 calc PR C 1 N3 N 0.2844(14) 0.3461(6) 0.3340(4) 0.027(2) Uani 0.65(4) 1 d P C 1 C3A C 0.3450(5) 0.4067(3) 0.3672(2) 0.0436(12) Uani 0.35(4) 1 d P C 2 H3A1 H 0.2856 0.4414 0.3469 0.052 Uiso 0.35(4) 1 calc PR C 2 H3A2 H 0.426 0.4289 0.3681 0.052 Uiso 0.35(4) 1 calc PR C 2 C4A C 0.3201(4) 0.3133(3) 0.2786(2) 0.0413(12) Uani 0.35(4) 1 d P C 2 H4A1 H 0.3961 0.3122 0.2601 0.05 Uiso 0.35(4) 1 calc PR C 2 H4A2 H 0.2635 0.3477 0.2559 0.05 Uiso 0.35(4) 1 calc PR C 2 N3A N 0.340(4) 0.3347(11) 0.3380(8) 0.033(6) Uani 0.35(4) 1 d P C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0311(3) 0.0284(3) 0.0150(2) -0.00211(19) 0.00073(16) -0.0019(2) Cl1 0.0431(7) 0.0377(7) 0.0290(6) -0.0052(5) 0.0052(5) 0.0026(5) N1 0.044(2) 0.028(2) 0.0165(17) -0.0007(15) 0.0027(15) -0.0013(17) N2 0.039(2) 0.034(2) 0.0175(17) -0.0031(16) 0.0073(15) -0.0003(17) N4 0.030(2) 0.040(2) 0.0238(18) -0.0097(16) 0.0046(14) -0.0060(17) N5 0.0280(19) 0.044(2) 0.0168(17) -0.0033(15) 0.0020(14) -0.0006(16) N6 0.029(2) 0.048(2) 0.0235(19) -0.0063(17) 0.0029(15) -0.0046(17) C1 0.037(3) 0.037(3) 0.021(2) 0.002(2) 0.0042(17) -0.002(2) C2 0.089(4) 0.031(3) 0.032(3) 0.000(2) 0.003(3) -0.016(3) C5 0.052(3) 0.053(4) 0.021(2) -0.002(2) 0.009(2) 0.003(2) C6 0.032(2) 0.031(2) 0.018(2) 0.0046(18) 0.0036(16) -0.0012(19) C7 0.036(3) 0.062(4) 0.030(2) -0.012(2) 0.011(2) -0.001(2) C8 0.031(3) 0.075(4) 0.031(3) -0.007(3) 0.0091(19) 0.000(2) C9 0.037(3) 0.061(4) 0.037(3) -0.015(3) 0.001(2) -0.011(2) C10 0.041(3) 0.058(3) 0.031(3) -0.018(2) 0.002(2) -0.010(2) C11 0.032(2) 0.032(3) 0.020(2) -0.0046(18) 0.0036(17) 0.0021(19) Cl1S 0.0629(10) 0.0812(12) 0.0738(11) -0.0103(9) 0.0148(8) 0.0122(8) Cl2S 0.147(2) 0.1100(19) 0.0919(16) 0.0089(14) 0.0114(14) 0.0013(15) Cl3S 0.1174(15) 0.0675(11) 0.0495(9) -0.0033(8) 0.0332(9) -0.0171(10) Cl4S 0.203(3) 0.0562(11) 0.0694(12) -0.0038(9) 0.0501(14) -0.0014(13) Cl5S 0.0594(9) 0.0814(12) 0.0571(9) -0.0085(8) -0.0003(7) 0.0195(8) C1S 0.038(3) 0.092(5) 0.065(4) -0.034(4) 0.010(3) -0.003(3) C2S 0.086(5) 0.058(4) 0.054(4) 0.007(3) 0.018(3) -0.008(3) C3S 0.041(4) 0.039(5) 0.112(7) 0 0.021(4) 0 C3 0.058(3) 0.040(3) 0.031(3) 0.009(2) -0.004(2) -0.009(2) C4 0.039(3) 0.062(3) 0.024(2) 0.004(2) 0.0083(19) -0.002(2) N3 0.024(6) 0.035(4) 0.022(3) 0.005(3) 0.007(3) 0.006(4) C3A 0.058(3) 0.040(3) 0.031(3) 0.009(2) -0.004(2) -0.009(2) C4A 0.039(3) 0.062(3) 0.024(2) 0.004(2) 0.0083(19) -0.002(2) N3A 0.051(16) 0.023(8) 0.030(7) -0.005(5) 0.022(9) -0.005(9) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 2.011(3) . ? Pd1 N1 2.011(3) 7_556 ? Pd1 N5 2.014(3) 7_556 ? Pd1 N5 2.014(3) . ? N1 C1 1.302(5) . ? N1 C2 1.483(6) . ? N2 C1 1.336(6) . ? N2 C11 1.436(6) . ? N2 C5 1.475(5) . ? N4 C6 1.340(5) . ? N4 C11 1.443(5) . ? N4 C10 1.479(6) . ? N5 C6 1.294(5) . ? N5 C7 1.487(6) . ? N6 C6 1.371(5) . ? N6 C9 1.461(6) . ? N6 C8 1.463(6) . ? C1 N3 1.363(10) . ? C1 N3A 1.375(18) . ? C2 C3 1.533(7) . ? C2 H2B 0.99 . ? C2 H2A 0.99 . ? C5 C4 1.531(7) . ? C5 H5B 0.99 . ? C5 H5A 0.99 . ? C7 C8 1.529(7) . ? C7 H7B 0.99 . ? C7 H7A 0.99 . ? C8 H8B 0.99 . ? C8 H8A 0.99 . ? C9 C10 1.535(7) . ? C9 H9B 0.99 . ? C9 H9A 0.99 . ? C10 H10B 0.99 . ? C10 H10A 0.99 . ? C11 H11B 0.99 . ? C11 H11A 0.99 . ? Cl1S C1S 1.773(7) . ? Cl2S C1S 1.739(7) . ? Cl3S C2S 1.734(6) . ? Cl4S C2S 1.742(7) . ? Cl5S C3S 1.773(5) . ? C1S H1S2 0.99 . ? C1S H1S1 0.99 . ? C2S H2S2 0.99 . ? C2S H2S1 0.99 . ? C3S Cl5S 1.773(5) 2_656 ? C3S H3S2 0.99 . ? C3S H3S1 0.99 . ? C3 N3 1.451(11) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? C4 N3 1.484(12) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 N1 180.0000(10) . 7_556 ? N1 Pd1 N5 87.55(14) . 7_556 ? N1 Pd1 N5 92.45(14) 7_556 7_556 ? N1 Pd1 N5 92.45(14) . . ? N1 Pd1 N5 87.55(14) 7_556 . ? N5 Pd1 N5 180.00(9) 7_556 . ? C1 N1 C2 106.1(4) . . ? C1 N1 Pd1 130.3(3) . . ? C2 N1 Pd1 123.6(3) . . ? C1 N2 C11 125.2(3) . . ? C1 N2 C5 109.0(4) . . ? C11 N2 C5 125.3(4) . . ? C6 N4 C11 124.5(3) . . ? C6 N4 C10 108.3(4) . . ? C11 N4 C10 124.9(3) . . ? C6 N5 C7 105.7(3) . . ? C6 N5 Pd1 130.3(3) . . ? C7 N5 Pd1 123.9(3) . . ? C6 N6 C9 107.2(4) . . ? C6 N6 C8 105.5(3) . . ? C9 N6 C8 126.2(4) . . ? N1 C1 N2 133.5(4) . . ? N1 C1 N3 114.7(6) . . ? N2 C1 N3 111.5(5) . . ? N1 C1 N3A 115.0(9) . . ? N2 C1 N3A 108.3(7) . . ? N1 C2 C3 104.6(4) . . ? N1 C2 H2B 110.8 . . ? C3 C2 H2B 110.8 . . ? N1 C2 H2A 110.8 . . ? C3 C2 H2A 110.8 . . ? H2B C2 H2A 108.9 . . ? N2 C5 C4 102.9(4) . . ? N2 C5 H5B 111.2 . . ? C4 C5 H5B 111.2 . . ? N2 C5 H5A 111.2 . . ? C4 C5 H5A 111.2 . . ? H5B C5 H5A 109.1 . . ? N5 C6 N4 133.1(4) . . ? N5 C6 N6 115.5(4) . . ? N4 C6 N6 111.3(4) . . ? N5 C7 C8 103.9(4) . . ? N5 C7 H7B 111 . . ? C8 C7 H7B 111 . . ? N5 C7 H7A 111 . . ? C8 C7 H7A 111 . . ? H7B C7 H7A 109 . . ? N6 C8 C7 100.2(4) . . ? N6 C8 H8B 111.7 . . ? C7 C8 H8B 111.7 . . ? N6 C8 H8A 111.7 . . ? C7 C8 H8A 111.7 . . ? H8B C8 H8A 109.5 . . ? N6 C9 C10 100.7(4) . . ? N6 C9 H9B 111.6 . . ? C10 C9 H9B 111.6 . . ? N6 C9 H9A 111.6 . . ? C10 C9 H9A 111.6 . . ? H9B C9 H9A 109.4 . . ? N4 C10 C9 101.5(3) . . ? N4 C10 H10B 111.5 . . ? C9 C10 H10B 111.5 . . ? N4 C10 H10A 111.5 . . ? C9 C10 H10A 111.5 . . ? H10B C10 H10A 109.3 . . ? N2 C11 N4 114.8(4) . . ? N2 C11 H11B 108.6 . . ? N4 C11 H11B 108.6 . . ? N2 C11 H11A 108.6 . . ? N4 C11 H11A 108.6 . . ? H11B C11 H11A 107.6 . . ? Cl2S C1S Cl1S 110.7(3) . . ? Cl2S C1S H1S2 109.5 . . ? Cl1S C1S H1S2 109.5 . . ? Cl2S C1S H1S1 109.5 . . ? Cl1S C1S H1S1 109.5 . . ? H1S2 C1S H1S1 108.1 . . ? Cl3S C2S Cl4S 111.4(4) . . ? Cl3S C2S H2S2 109.4 . . ? Cl4S C2S H2S2 109.4 . . ? Cl3S C2S H2S1 109.4 . . ? Cl4S C2S H2S1 109.4 . . ? H2S2 C2S H2S1 108 . . ? Cl5S C3S Cl5S 111.0(4) 2_656 . ? Cl5S C3S H3S2 109.4 2_656 . ? Cl5S C3S H3S2 109.4 . . ? Cl5S C3S H3S1 109.4 2_656 . ? Cl5S C3S H3S1 109.4 . . ? H3S2 C3S H3S1 108 . . ? N3 C3 C2 100.9(5) . . ? N3 C3 H3A 111.6 . . ? C2 C3 H3A 111.6 . . ? N3 C3 H3B 111.6 . . ? C2 C3 H3B 111.6 . . ? H3A C3 H3B 109.4 . . ? N3 C4 C5 100.9(5) . . ? N3 C4 H4A 111.6 . . ? C5 C4 H4A 111.6 . . ? N3 C4 H4B 111.6 . . ? C5 C4 H4B 111.6 . . ? H4A C4 H4B 109.4 . . ? C1 N3 C3 106.2(6) . . ? C1 N3 C4 106.6(8) . . ? C3 N3 C4 125.7(9) . . ? #===END